(19)
(11) EP 2 300 831 B1

(12) EUROPEAN PATENT SPECIFICATION

(45) Mention of the grant of the patent:
04.12.2013 Bulletin 2013/49

(21) Application number: 08774813.3

(22) Date of filing: 07.07.2008
(51) International Patent Classification (IPC): 
G01N 33/52(2006.01)
G01N 33/94(2006.01)
(86) International application number:
PCT/EP2008/058738
(87) International publication number:
WO 2010/003447 (14.01.2010 Gazette 2010/02)

(54)

METHOD FOR ON-SITE DRUG DETECTION IN ILLICIT DRUG SAMPLES

VERFAHREN ZUM ON-SITE-DROGENNACHWEIS BEI ILLEGALEN DROGENPROBEN

PROCEDE DE MARQUAGE CHIFFRE AUTOMATIQUE ET D'IDENTIFICATION DES LIQUIDES


(84) Designated Contracting States:
AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MT NL NO PL PT RO SE SI SK TR

(43) Date of publication of application:
30.03.2011 Bulletin 2011/13

(73) Proprietor: NARTEST INTERNATIONAL AS
12915 Tallinn (EE)

(72) Inventors:
  • BABICHENKO, Sergey
    EE12012 Tallinn (EE)
  • IVKINA, Tatjana
    Morrisville, NC 27560 (US)
  • PORYVKINA, Larisa
    EE12616 Tallinn (EE)
  • SOMINSKY, Vitaly
    Morrisville, NC 27560 (US)

(74) Representative: Ostrat, Jaak et al
Lasvet Patent & Trademark Agency Suurtüki 4A
10133 Tallinn
10133 Tallinn (EE)


(56) References cited: : 
WO-A-2005/111586
   
  • HILL LAUREN A ET AL: "A screening test for heroin based on sequential injection analysis with dual-reagent chemiluminescence detection." TALANTA 30 JUL 2008, vol. 76, no. 3, 16 April 2008 (2008-04-16), pages 674-679, XP022716059 ISSN: 1873-3573
  • ANDRE J C ET AL: "Application of synchronous excitation spectrofluorimetry to drug analysis." CLINICA CHIMICA ACTA; INTERNATIONAL JOURNAL OF CLINICAL CHEMISTRY 1 APR 1977, vol. 76, no. 1, 1 April 1977 (1977-04-01), pages 55-66, XP002510763 ISSN: 0009-8981
  • HUPKA Y ET AL: "HPLC with laser-induced native fluorescence detection for morphine and morphine glucuronides from blood after immunoaffinity extraction." INTERNATIONAL JOURNAL OF LEGAL MEDICINE MAY 2005, vol. 119, no. 3, May 2005 (2005-05), pages 121-128, XP002510764 ISSN: 0937-9827
  • MULÉ S J ET AL: "Semiautomated fluorometric assay for submicrogram quantities of morphine and quinine in human biological material." ANALYTICAL CHEMISTRY MAY 1971, vol. 43, no. 6, May 1971 (1971-05), pages 708-716, XP002510765 ISSN: 0003-2700
  • VENN R F ET AL: "Fast reliable assay for morphine and its metabolites using high-performance liquid chromatography and native fluorescence detection." JOURNAL OF CHROMATOGRAPHY 23 FEB 1990, vol. 525, no. 2, 23 February 1990 (1990-02-23), pages 379-388, XP008100605 ISSN: 0021-9673
  • NAKAMURA G R ET AL: "Kinetics of heroin deacetylation in aqueous alkaline solution and in human serum and whole blood." JOURNAL OF CHROMATOGRAPHY 2 JUL 1975, vol. 110, no. 1, 2 July 1975 (1975-07-02), pages 81-89, XP008100556 ISSN: 0021-9673 cited in the application
  • POLETTINI A ET AL: "Determination of opiates in hair. Effects of extraction methods on recovery and on stability of analytes." FORENSIC SCIENCE INTERNATIONAL 17 JAN 1997, vol. 84, no. 1-3, 17 January 1997 (1997-01-17), pages 259-269, XP002510766 ISSN: 0379-0738
  • BARRETT D A ET AL: "The effect of temperature and pH on the deacetylation of diamorphine in aqueous solution and in human plasma." THE JOURNAL OF PHARMACY AND PHARMACOLOGY JUL 1992, vol. 44, no. 7, July 1992 (1992-07), pages 606-608, XP008100564 ISSN: 0022-3573
   
Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention).


Description

FIELD OF THE INVENTION



[0001] The invention relates to the field of drug detection in illicit drug samples. In the sense of the present invention, illicit drug sample is a product that may contain in addition to illicit drug adulterants and/or diluents (also denominated as cutting agents) used for secret substitution of a more expensive illicit drug with cheaper substances or for disguising the existence of an illicit drug. More particularly the invention relates to a method based on fluorescence in solution and specifically on the Spectral Fluorescence Signatures (SFS) technology, allowing detection of Heroin and Morphine and enabling increase of sensitivity of Heroin detection and of selectivity of Heroin and Morphine differentiation in illicit drug samples.

BACKGROUND OF THE INVENTION



[0002] A system and a method for on-site drug detection and quantification based on the Spectral Fluorescence Signatures (SFS) technology are disclosed in WO2005111586. The system of this invention consists of an ultraviolet-visible light source, a condenser/filter assembly with filter drive, an excitation monochromator with diffraction grating drive, a reference photo-detector, a cell assembly for liquid, solid and powder samples, an absorption photo-detector, an emission monochromator with diffraction grating drive, and an emission photo-detector. A microcontroller unit is provided for device controlling, data processing, and communication with an external computer via different link types. The detection and quantification of illicit drugs in the analyzed sample are provided by measuring simultaneously the emission spectra of fluorescence at every step of excitation wavelength in selected and fixed excitation, emission and absorption spectral windows in a way to cover specific excitation, emission fluorescence and absorption spectral ranges of all major drugs, adulterants and diluents; and processing the united result in a computer system based on combination of preliminary prepared spectral library and specialized software consisting of identification, interaction verification and automatic calibration modules.

[0003] A system and a method of analysis of illicit drug samples disclosed in WO2005111586 are limited in detection by the concentration of the substances of interest, in particular Heroin. Due to low fluorescence efficiency of Heroin and interfering influence of adulterants and diluents, the specific patterns in SFS structure caused by said substances at certain concentration of Heroin are not recognized by the expert system.

[0004] WO 2008040386 discloses a method for on-site drug detection in illicit drug samples enabling preferably Cocaine drug detection in street samples containing in addition to Cocaine also adulterants and/or diluents. The method provides preparing of the liquid street sample, taking of an aliquot of said sample, its analysis with help of SFS (Spectral Fluorescence Signatures) technology, fixing the result of analysis as a reference value, the subsequent acidification of the liquid sample, taking an aliquot of the acidified liquid sample and its analysis with help of SFS technology, fixing the result of analysis and comparing said result with the reference value. The result of comparison enables to differentiate between Cocaine Base and Cocaine hydrochloride in the street sample. On the essence, the subject invention uses an additional chemical reaction for modifying the sample before performing the second measurement. This chemical reaction enables to raise the intensity of the sample for analysis with SFS technology by way of converting Cocaine Base to Cocaine hydrochloride.

[0005] The above method as such cannot be used for detection of Heroin in illicit drug samples because the simple acidification of a sample and comparision the results of the measurement of the sample before and after acidification does not grant the reliable results due to the specific chemical qualities of Heroin and existence of adulterants and/or diluents in the sample.

[0006] Hill et al (2008, Talanta, 76, 674-679) discloses a method for drug detection, namely heroin and morphine, based on sequential injection technology comprising allotting the sample in two aliquots, one of which is directly diluted in acetic acid ("unhydrolysed" sample). The second aliquot is treated with NaOH to rapidly convert the heroin to morphine and then treated with acetic acid solution. Chemiluminescent measurement of morphine is performed in both aliquots after treatment with a permanganate reagent.

[0007] Andre et al (1977, Clin Chim Acta, 55-66) describes detection of pure drugs in a solvent by synchronous excitation spectrofluorimetry.

[0008] Hupta et al (2005, Int J Legal Med, 119, 121-128) and Venn et al (1990, J Chrom, 525, 379-388) register integral fluorescence intesity after drug separation by HPLC.

[0009] Mule et al (1971, Anal Chem, 43(6), 708-711) performs an extraction of morphine followed by fluorimetric deteciton.

[0010] At the same time, the need for a technical solution, which increases the sensitivity and selectivity of on-site analysis related to Heroin and Morphine detection in a mixture with cutting agents (adulterants and diluents) is mandated by the legal requirements in illicit drug distribution prevention. The current sentencing structure for Heroin offences (United States Sentencing Commission. Guidelines Manual. 2006) in the Schedule I of the referenced document provides for the less than 5 g of Heroin the same sentences as for about 25 g of Cocaine. Liability for seized 1 g of Heroin is equal according to this document to 1 kg of Marijuana (Marihuana). Sentencing structure for Morphine offences has been put in the Schedule II. Liability for seized 1 g of Morphine is equal according to the same document to 500 g of Marijuana (Marihuana). The cited documents illustrate necessity to provide reliable and selective detection of Heroin and Morphine to fight effectively against this illegal drugs trafficking and abuse.

SUMMARY OF INVENTION



[0011] In its broadest sense, the invention pertains to subject-matter as defined in the appended claims.

[0012] Resulting from the drawbacks of the known technical solutions, the first objective of the present invention is to provide a method for on-site drug detection in illicit drug samples using SFS analysis enabling reliable detection of Heroin and Morphine in a sample.

[0013] Another objective of the present invention is to increase the sensitivity and selectivity of SFS analysis for Heroin detection in the mixtures with cutting agents.

[0014] Further objective of the present invention is to ensure the safe differentiation of Heroine and Morphine in a sample. To solve the problem of detection limits due to low fluorescence efficiency of Heroin and interfering influence of adulterants and diluents, a chemical conversion of Heroin to Morphine suitable for on-site use was elaborated by the inventors. Morphine has higher fluorescence efficiency than Heroin, its spectral patterns in SFS structure are different by shape and position compared to Heroin, and therefore the presence of Morphine in converted sample can serve as a good indicator of Heroin presence in initial sample. Conversion of Heroin to Morphine in alkali has been applied.

[0015] According to this procedure false positive detection of Heroin may occur if Morphine is present in drug sample as an independent component or as a result of partial Heroin self-conversion. Therefore differentiation of Heroin in presence of Morphine and exclusion of false positive results in drug sample is required. It is provided by detection of Morphine presence in drug sample before applying the procedure of chemical conversion to the sample.

[0016] For achieving the above objectives, the suggested method for on-site drug detection in illicit drug samples is based on the analysis by Spectral Fluorescence Signatures (SFS) technology and is provided by executing the following steps:

preparing a liquid sample from of a street sample for analysis;

allotting the liquid sample into two equal aliquot samples, first of which is the reference sample and the second one is the main sample;

prior to the measurement, first the Hydrochloric acid and then Sodium hydroxide are added into the reference sample;

the reference sample is introduced in the into the measuring cell of a SFS device;

the measurement of SFS of the reference sample is performed;

the presence of specific spectral pattern of Morphine in the measured SFS of the reference sample is detected and the value of SFS intensity at the specific spectral point is fixed;

the value of SFS intensity of the reference sample at the specific spectral point is considered as a reference value;

prior to the measurement, Sodium hydroxide is added to the main sample for conversion of hereoin into morphine to provide the increase of the value of SFS intensity at the specific point of the special pattern of morphine;

after expiring the time limit provided for hydrolysis of the main sample, Hydrochloric acid is added to the sample in order to stop the hydrolysis process;

the main sample is introduced in the into the measuring cell of a SFS device;

the measurement of SFS of the main sample is performed;

the presence of specific spectral pattern of Morphine in the measured SFS of the main sample is detected and the value of SFS intensity at the specific spectral point is fixed;

the reference value and the value of SFS intensity of the main sample at the specific spectral point are compared, and,

if the reference value and the value of SFS intensity of the main sample at the specific spectral point both equal zero, existence neither Heroin nor Morphine in the street sample is considerd proved;

if the reference value differs from zero, the existence of Morphine in the street sample is considered proved;

if the value of SFS intensity of the main sample at the specific spectral point equals to the reference value lacking of Heroin in the street sample is considered proved;

if the value of SFS intensity of the main sample at the specific spectral point exceeds the reference value, the existence of Heroin in the street sample is considered proved.



[0017] The SFS specific spectral point for comparison is 285/345 nm.

[0018] The preferred time limit provided for conversion of Heroin to Morphine is 15 minutes.

BRIEF DESCRIPTION OF DRAWINGS



[0019] 
Flow-Chart 1.
The flow-chart of the method for detection of Heroin and Morphine in the illicit drug samples
Fig. 1.
Intensity of Heroin hydrochloride fluorescence at the specific point 285/340-345 nm in the concentration range of 3.9 - 1000 mg/l in water with reagents before (reagents added in the reverse order to prevent hydrolysis) and after conversion to Morphine (due to hydrolysis) - the results of measurement of the reference sample and the main one.
Fig.2.
Intensity of Morphine sulphate fluorescence at the specific point 285/340-345 nm in the concentration range of 0.488 - 2000 mg/l in water with reagents before (reagents added in the reverse order to prevent hydrolysis) and after hydrolysis - the results of measurement of the reference sample and the main one.
Fig.3.
Spectral Fluorescence Signatures of Morphine, Heroin, and Heroin in the mixture with Procaine before (reference samples) and in the process of conversion (hydrolysis).

DETAILED DESCRIPTION OF THE INVENTION



[0020] According to the present invention, the first step of the method is preparing the liquid sample for analysis. For this purpose the sampled amount of dry sample as a powder taken by a sampling tool (e.g. spatula) is transferred into purified water, and water with powder is mixed to assist dilution of the powder in water. Usually 20 mg of a powder is diluted in 10 ml of purified water but it has been revealed that the amount of the power may vary from 18 to 23 mg, this variation does not influence the results of the further measurements.

[0021] After that, the liquid sample is divided into 2 equal aliquots - the reference sample and the main one. Sodium hydroxide is added to the main sample in order to convert possibly present Heroin to Morphine by way of hydrolysis process. The amount of the added Sodium hydroxide is 3-5 drops. Conversion is stopped after 15 minutes by addition of 3-5 drops of Hydrochloric acid The time of the conversion is substantiated by the experiments performed by the inventors - with reference to Fig. 4 it is evident that after passing of 15 minutes hydrolysis of the main sample, the Spectral Fluorescence Signature of Heroin has been transferred to the SFS of Morphine. Even by the presence of cutting agents in the sample (e.g. Procaine as one of the wide-spread cutting agent in the sized Heroin samples) the above time-limit is sufficient to reach the SFS of the sample very near to the SFS of Morphine and acceptable for the SFS measurement. Thus the time-limit found by the inventors is sufficient to provide Heroin detection in different mixtures.

[0022] To the reference sample, 3-5 drops of Hydrochloric acid is added to prevent conversion of possibly present Heroin, and 3-5 drops of Sodium hydroxide after it to keep contents of two aliquots the same. Affecting the reference sample with the chemical substances mentioned above is necessary for achieving the more reliable results of measurement - due to the possible existence adulterants and diluents in the street sample, the both samples to be measured have to be affected by the identical additional chemicals in order to prevent the possible distortions which may arise when only the main sample is additionally processed with Sodium hydroxide and Hydrochloric acid,

[0023] The reference sample is introduced into the measurement cell of the device according to W02005111586 and SFS of the aliquot of liquid sample is measured. Upon acquisition of the SFS, the expert system of the device based on the spectral patterns recognition in measured SFS provides detection of Morphine in the sample, and registers the intensity value at the specific point (285/345 nm) if Morphine detected.

[0024] The procedure of Heroin conversion for on-site use must be simple and fast. There are at least two methods of Heroin conversion into Morphine: acid and alcali hydrolysis. The experiments completed by inventors have revealed that the acid hydrolysis [D. Zhang et al] requires heating of the sample for efficient conversion in enough short time. As heating complicates the realization of procedure on-site, this method has been rejected. Alcali hydrolysis using Sodium hydroxide [G. Nakamura] has been tested and accepted as enough efficient and simple method of Heroin conversion to Morphine. Sodium hydroxide concentration influences speed of hydrolysis but should be as low as possible for on-site use because lower concentration decreases potential risk for performers of the process. Sodium hydroxide in the cited works has been used in 2N or 1N concentrations but the inventors have determined that 0.5N is enough to provide conversion of Heroin into Morphine within acceptable time interval for on-site use.

[0025] After possibly present Heroin has passed the established time for conversion into Morphine, and the Hydrochloric acid is added to the sample to stop the further conversion, the main sample is introduced into the measurement cell of the device, and the SFS of the sample is measured. Upon acquisition of the SFS, the expert system of the device provides the detection of Morphine in the sample, registers the intensity value at the specific point of the SFS if Morphine detected, and compares the intensity value with that of the reference sample.

[0026] Presence of Morphine in the reference sample may be due to a spontaneous hydrolysis of Heroin in the seized sample before analysis. Morphine may also be present independently on Heroin. If Morphine is detected in the reference sample and in the main sample after hydrolysis, and the fluorescence intensity at the specific point of SFS is increased, it is evidence of Heroin presence in the analyzed sample (Fig.2). There is no other source of such result because fluorescence of Morphine is not increased after hydrolysis (Fig.3). Only increase of Morphine concentration due to conversion from Heroin may be the origin of SFS intensity rise in the described procedure.

[0027] Accordingly, absence of Morphine in the reference sample and its presence in the main sample after hydrolysis is the evidence of Heroin presence in the analyzed drug sample.

[0028] If Morphine is detected in the reference sample and in the main sample after hydrolysis but the fluorescence intensity of the main sample at the specific point of SFS is not increased, it is evidence of Morphine presence and absence of Heroin in the analyzed drug sample.

[0029] A step-by-step performance of the present invention is shown below.
  1. 1. Transferring a proper amount of drug sample into a test container with a rational volume of pure water.
  2. 2. Giving the amount of drug sample to be dissolved at possible instant within 3 minute time interval and allowing any insoluble materials settle to the bottom of the container.
  3. 3. Division of the liquid sample for two equal samples (reference sample and main one).
  4. 4. Addition of Hydrochloric acid to the reference sample
  5. 5. Addition of Sodium hydroxide to both samples
  6. 6. Leaving the main sample for 15 minutes (hydrolysis for converting of Heroin to Morphine)
  7. 7. Taking a proper volume of the liquid from the reference sample and placing it into the measurement cell of the SFS measuring device according to W02005111586.
  8. 8. Measuring the SFS of the reference sample and detecting spectral pattern of Morphine if present. The result of the measurement of the intensity of Morphine fluorescence at the specific point of SFS serves as the reference value.
  9. 9. After passing of 15 minutes, adding Hydrochloric acid to the main sample for stopping the hydrolysis process.
  10. 10. Taking a proper volume of the liquid from the main sample and placing it into the measurement cell of the SFS measuring device according to W02005111586.
  11. 11. Measuring the SFS of the main sample and detecting specific spectral pattern of Morphine if present. The result of the measurement of the intensity of Morphine fluorescence at the specific point of SFS of the main sample will be compared with the reference value.
  12. 12. Comparing the intensities of Morphine fluorescence of the reference and main samples provided that the intensity of Morphine fluorescence of the reference sample is detected. Higher intensity of the fluorescence of the main sample indicates that Heroin is present in analyzed drug sample. And on the contrary, lower or unchanged intensity of the fluorescence of the main sample indicates that only Morphine is present in analyzed drug sample. Absence of Morphine in the reference sample and its appearance in the main sample is evidence of Heroin presented in analyzed drug sample. Absence of Morphine fluorescence in the both samples indicates that neither Morphine nor Heroin are present in analyzed drug sample.


[0030] The table below illustrates the results of detection of Heroin in street samples according to the present invention. As in the street samples ## 2, 3 and 15 the difference between the reference value and the the result of the measurement of SFS of the main sample in the SFS specific spectral point is unessential, it may be concluded that those street samples do not contain Heroin. For all the remaining street samples the adversative conclusion can be made.
Street sample # Morphine detected before hydrolysis Morphine detected after hydrolysis Increase of intensity, %
Intensity (a.u.) at 285/345 nm Intensity (a.u.) at 285/345 nm
1 75.5 209.8 +173
2 1094.0 1275.7 +21
3 1643.5 2534.8 +54
4 718.3 2447.4 +241
5 140.0 1279.0 +814
6 436.0 2242.9 +414
7 499.4 2890.2 +479
8 297.3 2849.0 +858
9 1110.3 2431.3 +119
10 457.4 2441.6 +478
11 364.7 2981.0 +704
12 272.0 2727.8 +903
13 308.2 3485.4 +1031
14 447.9 2871.9 +542
15 497 836 +48
16 440.1 2904.3 +560


[0031] The procedure of Heroin detection can be provided automatically by Expert system analyzing the SFS. Such expert system considers not only the shape and position of Morphine spectra but their intensities and appearance of Morphine spectral pattern or increase of its fluorescence intensity.

[0032] The disclosed embodiment of the invention does not determine its scope of protection, but shows only one of variants of its realization within the scope defined by claims.

REFERENCES



[0033] 

WO2005111586. S.Babichenko, E.Erme, T.Ivkina, L.Poryvkina, V.Sominsky. A PORTABLE DEVICE AND METHOD FOR ON-SITE DETECTION AND QUANTIFICATION OF DRUGS.

WO2008040386. S.Babichenko, T.Ivkina, L.Poryvkina, V.Sominsky. METHOD FOR ON-SITE DRUG DETECTION IN ILLICIT DRUG SAMPLES.

D. Zhang et al. Origin differentiation of Heroin sample and its acetylating agent 13C isotope ratio mass spectrometry. Eur. J. Mass Spectrom. 11, 277-285 (2005).

G. Nakamura, T. Ukita. Codeine to Morphine Ratio of Illicit Heroin Hydrolysates. UNODC - Bulletine on Narcotics, 1963,1-008; G. Nakamura and J. Thornton. KINETICS OF HEROIN DEACETYLATION IN AQUEOUS ALCALINE SOLUTION AND IN HUMAN SERUM AND WHOLE BLOOD. Journal of Chromatography, 110: 81-89 (1975).






Claims

1. Method for on-site drug detection in illicit drug samples basing on the analysis performed by the Spectral Fluorescence Signatures (SFS) technology, providing preparing a liquid sample from of a street sample for analysis;
the measurements of the SFS of a sample;
making conclusions on the base of the results of the measurements,
characterized in that
the liquid sample is allotted into two aliquot samples, first of which is a reference sample and the second one is the main sample;
prior to the measurement, first the Hydrochloric acid and then Sodium hydroxide are added into the reference sample;
the reference sample is introduced into the measuring cell of a SFS device;
the measurement of the SFS of the reference sample is performed;
the presence of spectral pattern of Morphine in the measured SFS of the reference sample is detected and the value of SFS intensity at the selected spectral point of SFS is fixed;
the value of the SFS intensity of the reference sample at the selected spectral point of SFS is considered as a reference value;
prior to the measurement, Sodium hydroxide is added to the main sample for conversion of Heroin into Morphine to provide the use of the increased value of SFS intensity of the spectral pattern of Morphine at the selected spectral point of SFS.;
after expiring the time limit provided for hydrolysis of the main sample, Hydrochloric acid is added to the main sample in order to stop the hydrolysis process;
the main sample is introduced into the measuring cell of a SFS device;
the measurement of the SFS of the main sample at the selected spectral point of SFS is performed;
the presence of spectral pattern of Morphine in the measured SFS of the main sample is detected and the value of SFS intensity at the selected specific spectral point of SFS is fixed;
the reference value and the value of SFS intensity of the main sample at the specific spectral point of SFS are compared, at that
the selected spectral point of SFS is determined at the excitation wavelength 285 nm and emission wavelengths 340-345 nm.
 
2. Method for on-site drug detection in illicit drug samples according to claim 1, characterized in that if the result of the comparison reveals the reference value and the value of SFS intensity of the main sample at the selected spectral point of SFS both being equal to zero, existence neither Heroin nor Morphine in the street sample is considered proved.
 
3. Method for on-site drug detection in illicit drug samples according to claim 1, characterized in that if the result of the comparison reveals the reference value differing from zero, the existence of Morphine in the street sample is considered proved.
 
4. Method for on-site drug detection in illicit drug samples according to claim 1, characterized in that if the result of the comparison reveals the reference value being equal to the value of SFS intensity of the main sample at the selected spectral point of SFS, lacking of Heroin in the street sample is considered proved.
 
5. Method for on-site drug detection in illicit drug samples according to claim 1, characterized in that if the result of the comparison reveals the value of SFS intensity of the main sample at the selected spectral point of SFS exceeding the reference value, the existence of Heroin in the street sample is considered proved.
 
6. Method for on-site drug detection in illicit drug samples according to claim 1, characterized in that for preparing a liquid sample, a dry sample is dissolved in purified water.
 
7. Method for on-site drug detection in illicit drug samples according to claim 6, characterized in that as purified water distilled water is used.
 
8. Method for on-site drug detection in illicit drug samples according to claim 1, characterized in that the amount of Hydrochloric acid and Sodium hydroxide to be added to the samples is 3-5 drops.
 
9. Method for on-site drug detection in illicit drug samples according to claim 1, characterized in that the time limit provided for hydrolysis of the main sample is up to 15 minutes.
 


Ansprüche

1. Verfahren zum Drogennachweis vor Ort von illegalen Drogenproben basierend auf der Analyse mit der Spektralfluoreszenzsignatur (SFS) Technologie, umfassend die Schritte:

Vorbereitung einer Flüssigkeitsprobe von einer Straßenprobe zur Analyse;

die Messung von SFS einer Probe;

Schlüsse auf der Basis der Messergebnisse ziehen,

dadurch gekennzeichnet, dass

die Flüssigkeitsprobe wird in zwei aliquote Proben geteilt, die erste davon ist eine Vergleichsprobe und die zweite ist die Hauptprobe;

vor der Messung, werden zuerst die Chlorwasserstoffsäure und dann die Natronlauge der Vergleichsprobe hinzugefügt;

die Vergleichsprobe wird in die Messzelle eines SFS-Gerätes eingeführt;

die Messung der Vergleichsprobe wird vom SFS durchgeführt;

das Vorhandensein von spektralen Spuren von Morphium in der gemessenen SFS der Vergleichsprobe wird erkannt und der Wert der SFS Stärke am ausgewählten spektralen Punkt der SFS wird bestimmt;

der Wert der SFS Stärke der Vergleichsprobe am ausgewählten spektralen Punkt der SFS wird als Referenzwert betrachtet;

vor dem Messen, Natronlauge wird zur Hauptprobe zur Umwandlung von Heroin in Morphium hinzugefügt, um den gesteigerten Wert der SFS Intensität der spektralen Morphiumprobe am ausgewählten spektralen Punkt der SFS zu nutzen;

nach dem Ablauf des vorgegebenen Zeitlimits für die Hydrolyse der Hauptprobe, Chlorwasserstoffsäure wird zur Hauptprobe hinzugefügt um den Hydrolyseprozess zu stoppen;

die Hauptprobe wird in die Messzelle eines SFS-Gerätes eingeführt;

die Messung des SFS der Hauptprobe am ausgewählten spektralen Punkt der SFS wird durchgeführt;

das Auftreten von spektralen Spuren von Morphium in der gemessenen SFS der Hauptprobe wird erkannt und der Wert der SFS Stärke am ausgewählten spektralen Punkt der SFS wird bestimmt;

der Referenzwert und der Wert der SFS Intensität der Hauptprobe am spezifischen spektralen Punkt der SFS werden verglichen, daran,

dass der ausgewählte spektrale Punkt der SFS an der Speisung der Wellenlänge 285 nm und der Emissionswellenlänge 340-345 mm bestimmt wird.


 
2. Verfahren eines Drogennachweises vor Ort von illegalen Drogenproben nach Patentanspruch 1, dadurch gekennzeichnet, dass den Ergebnisvergleich vom Referenzwert und dem Wert der SFS Intensität der Hauptprobe am ausgewählten spektralen Punkt der SFS zeigt indem sie beide identisch gleich Null sind, wird weder die Existenz von Herein noch von Morphium in der Straßenprobe als bewiesen anerkannt.
 
3. Verfahren eines Drogennachweises vor Ort von illegalen Drogenproben nach Patentanspruch 1, dadurch gekennzeichnet, dass wenn beim Ergebnisvergleich der Referenzwert von Null abweicht, gilt das Vorhandensein von Morphium in der Straßenprobe als bewiesen.
 
4. Verfahren eines Drogennachweises vor Ort von illegalen Drogenproben nach Patentanspruch 1, dadurch gekennzeichnet, dass wenn beim Ergebnisvergleich der Referenzwert gleich ist wie der Wert der SFS Intensität der Hauptprobe am ausgewählten spektralen Punkt der SFS, gilt das Vorhandensein von Heroin in der Straßenprobe als nicht erwiesen.
 
5. Verfahren eines Drogennachweises vor Ort von illegalen Drogenproben nach Patentanspruch 1, dadurch gekennzeichnet, dass wenn beim Ergebnisvergleich der Referenzwert dem Wert der SFS Intensität der Hauptprobe am ausgewählten spektralen Punkt der SFS überschritten wird, gilt das Vorhandensein von Heroin in der Straßenprobe als erwiesen.
 
6. Verfahren zum Drogennachweis vor Ort von illegalen Drogenproben nach Patentanspruch 1, dadurch gekennzeichnet, dass in der Vorbereitung einer Flüssigkeitsprobe, eine Trockenprobe wird in gereinigtes Wasser aufgelöst.
 
7. Verfahren eines Drogennachweises vor Ort von illegalen Drogenproben entprechend des Patentanspruch 6, dadurch gekennzeichnet, dass destilliertes Wasser als aufbereitetes Wasser verwendet wird.
 
8. Verfahren zum Drogennachweis vor Ort von illegalen Drogenproben entsprechend des Patentanspruch 1, dadurch gekennzeichnet, dass 3-5 Tropfen Chlorwasserstoffsäure und Natronlauge zu den Proben hinzugefügt werden sollen.
 
9. Verfahren zum Drogennachweis vor Ort von illegalen Drogenproben entsprechend Patentanspruch 1, dadurch gekennzeichnet, dass das vorgegebene Zeitlimit für die Hydrolyse der Hauptprobe bis zu 15 Minuten beträgt.
 


Revendications

1. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites se basant sur l'analyse effectuée par la technologie des Signatures Spectrales de Fluorescence (SFS), fournissant
la préparation d'un échantillon liquide à partir d'un échantillon de rue pour l'analyse;
les mesures de la SFS de l'échantillon;
tirer des conclusions sur la base des résultats des mesures,
caractérisé en ce que
l'échantillon liquide est réparti en deux échantillons aliquotes, dont le premier est un échantillon de référence et le second est l'échantillon principal;
avant la mesure, d'abord l'acide chlorhydrique, puis l'hydroxyde de sodium sont ajoutés à l'échantillon de référence;
l'échantillon de référence est introduit dans la cellule de mesure d'un dispositif SFS;
la mesure de la SFS de l'échantillon de référence est effectuée;
la présence de motif spectral de Morphine dans le SFS mesurées de l'échantillon de référence est détecté et la valeur d'intensité de SFS au niveau du point spectral sélectionné du SFS est fixé;
la valeur de l'intensité de SFS de l'échantillon de référence au niveau du point spectral sélectionné du SFS est considérée comme une valeur de référence;
avant la mesure, l'hydroxyde de sodium est ajouté à l'échantillon principal pour la conversion de l'héroïne en morphine pour permettre l'utilisation de la valeur augmentée de l'intensité de la SFS de motif spectral de morphine au niveau du point spectral sélectionné du SFS;
après l'expiration du délai prévu pour l'hydrolyse de l'échantillon principal, l'acide chlorhydrique est ajouté à l'échantillon principal afin d'arrêter le processus d'hydrolyse;
l'échantillon principal est introduit dans la cellule de mesure d'un dispositif SFS;
la mesure de la SFS de l'échantillon principal au niveau du point spectral sélectionné du SFS est effectuée;
la présence de motif spectral de morphine dans le SFS mesurées de l'échantillon principal est détecté et la valeur d'intensité de SFS au niveau du point spectral spécifique sélectionné du SFS est fixé;
la valeur de référence et la valeur de l'intensité de SFS de l'échantillon principal au niveau du point spectral spécifique sélectionné du SFS sont comparées,
le point spectral sélectionné du SFS est déterminée à la longueur d'onde d'excitation de 285 nm et les longueurs d'onde d'émission de 340 à 345 nm.
 
2. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites selon la revendication 1, caractérisé en ce que si le résultat de la comparaison fait apparaître la valeur de référence et la valeur de l'intensité de SFS de l'échantillon principal au niveau du point spectral sélectionné du SFS étant tous deux égaux à zéro, l'absence de héroïne et de morphine dans l'échantillon de rue est considérée comme prouvée.
 
3. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites selon la revendication 1, caractérisé en ce que si le résultat de la comparaison fait apparaître la valeur de référence à une différence de zéro, l'existence de Morphine dans l'échantillon de rue est considérée comme prouvée.
 
4. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites selon la revendication 1, caractérisé en ce que si le résultat de la comparaison fait apparaître la valeur de référence étant égale à la valeur de l'intensité de SFS de l'échantillon principal au niveau du point spectral sélectionné du SFS, l'absence d'héroïne dans l'échantillon de rue est considérée comme prouvée.
 
5. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites selon la revendication 1, caractérisé en ce que si le résultat de la comparaison fait apparaître la valeur de l'intensité de SFS de l'échantillon principal au niveau du point spectral sélectionné du SFS excédant la valeur de référence, l'existence de l'héroïne dans l'échantillon de rue est considérée comme prouvée.
 
6. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites selon la revendication 1, caractérisé en ce que pour la préparation d'un échantillon liquide, l'échantillon sec est dissous dans de l'eau purifiée.
 
7. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites selon la revendication 6, caractérisé en ce qu'en tant que l'eau purifiée, l'eau distillée est utilisée.
 
8. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites selon la revendication 1, caractérisé en ce que la quantité d'acide chlorhydrique et d' hydroxyde de sodium à ajouter à l'échantillon est de 3 à 5 gouttes.
 
9. Procédé pour la détection sur place de drogues dans des échantillons de drogues illicites selon la revendication 1, caractérisé en ce que le délai prévu pour l'hydrolyse de l'échantillon principal est jusqu'à 15 minutes.
 




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Cited references

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